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7-(3-t-Butoxycarbonylamino-4-methyl-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid → 7-(3-Amino-4-methyl-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

HRID 580573
ノート
印刷プレビュー

反応式

HRID 580573 の反応式
C(OC([NH:8][CH:9]1[CH:13]([CH3:14])[CH2:12][N:11]([C:15]2[C:24]([Cl:25])=[C:23]3[C:18]([C:19](=[O:32])[C:20]([C:29]([OH:31])=[O:30])=[CH:21][N:22]3[CH:26]3[CH2:28][CH2:27]3)=[CH:17][C:16]=2[F:33])[CH2:10]1)=O)(C)(C)C>CO.Cl>[NH2:8][CH:9]1[CH:13]([CH3:14])[CH2:12][N:11]([C:15]2[C:24]([Cl:25])=[C:23]3[C:18]([C:19](=[O:32])[C:20]([C:29]([OH:31])=[O:30])=[CH:21][N:22]3[CH:26]3[CH2:28][CH2:27]3)=[CH:17][C:16]=2[F:33])[CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 139330937-(3-t-Butoxycarbonylamino-4-methyl-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

生成物 1

HCID 139330957-(3-Amino-4-methyl-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid収率 25.3%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

実験手順

7-(3-t-Butoxycarbonylamino-4-methyl-1-pyrrolidinyl)-8-chloro-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (0.35 g) was dissolved in the mixture of methanol (5 ml) and concentrated hydrochloric acid (5 ml) and stirred at room temperature for 30 minutes. After the reacting mixture was concentrated under reduced pressure, the resulting residue was dissolved in ethanol (10 ml) and neutralized with concentrated aqueous ammonia. The resulting precipitate was collected by filtration, washed with water and recrystallized from chloroformmethanol-concentrated aqueous ammonia to give the title compound (0.07 g) as pale yellow powder, mp 231°-234° C.

後処理

  1. concentrationAfter the reacting mixture was concentrated under reduced pressure
  2. dissolutionthe resulting residue was dissolved in ethanol (10 ml) and neutralized with concentrated aqueous ammonia
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with water
  5. customrecrystallized from chloroformmethanol-concentrated aqueous ammonia

出典と根拠

ORDレコード
ord-77fdf73eb585441895742b6ccae3bd55
出典データセット
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04753953

反応ノート

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